Electrolytic apparatus



V. M. WEAVER.

ELECTROLYTIC APPAR ATUS. APPLICATION HLED my 9.191s.

1,329,315, Patented Jan. 27,1920.-

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Victor M. Weaver By W M v. M. WEAVER.

ELECTROLYHC APPARATUS. APPLICATION FILED JULY 9- I915- Patented Jan. 27,1920.

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V. M. WEAVER.

ELECTROLYTIC APPARATUS.

APPLICATION FILED JULY 9.1915.

Patented Jan. 27, 1920.

4 SHEETSSHEET 4- JEUUGTDIIOT Water Wmver poses hereinafter pointed out.

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umrnn STATES PATEN OFFICE.

VICTOR M. WEAVER, OF HARRISBURG,"PENNSYLVANIA, ASSIGNOR T0 WEAVER ICOMPANY, A CORPORATION OF WISCONSIN.

ELECTROLYTIC APPARATUS.

Specification of Letters Patent.

Original application filed Auguste, 1914, Serial No. 858,001. Dividedand application filed January 11,

1915, Serial No. 286. Divided and this application filed To all whom itmay concern Be it known that I, VICTOR M. WEAVER, a citizen of theUnited States, residing at arrisburg, in the county of Dauphin and Stateof Pennsylvania,

trolytic Apparatus,.of which the following is a' full, clear concise,and exact description, reference eing had to the fccompanying drawings,forming a part 0 this specification.

My invention relates to apparatus for car rying out electrolyticprocesses and steps in processes and contemplates a generallySlIIlplified and eflicient structure wherein the action may effectivelybe carried on. One important feature of my invention lies in the meansfor feeding the material to be treated and the arrangement of theelements. A

further feature of my invention lies in the sealed construction which Iprovide fon-pur- It will be clear to art that my invention will admit ofbroader application than the; specific uses which I shall describe as aninstance of its employment. In order to simplify this description Ishall describe'my apparatus as employed in carrying out a process ofsecuring aluminum from aluminum chlorid.

This application is divisional from m co-pending application, Serial No.286 filed .January 11, 1915, which in turn is divisional from myco-pending application, Serial No. 858,001, filed August 22, 1914,'whichis concerned with a process and apparatus for winning metals and which,in its'more specific aspects, relates to the treatment of clay in orderto secure the aluminum and the silicon therefrom.

In order to instruct those skilled in the art, I shall now proceed witha specific description of my invention as utilized in my process ofsecuring aluminum and silicon have invented a certain new and usefulImprovement in Elec- July 9,1915. Serial N 38,858.

from clay, and shall refer to and describe the various parts of theapparatus and the various stages in the process in detail, in order thatI may make a complete and intelligent disclosure.

In the treatment of clay, I break up the compound by the use of chloringas so as to produce aluminum chlorid and silicon tetrachlorid, thisaction being carried on under specialrestrictions and conditions, aswill later be more fully described. With the aluminum'chlorid thusproduced, the next step, so far as this particular part of the processis concerned, is to secure the by electrolysis under certain conditionsand restrictions calculated to effect an advantageous and continuousprocess. I charge the aluminum chlorid into an electrolyzing bathpreferably containing melted sodium chlorid, and the consequentelectrolysis separates the aluminum from the chlorin, so thatthe formermay be tapped away from the sodium chlorid, while the latter may beconducted to astorage tank for further use. It is important in thisconnection that in carrying out my process I keep the electrolytic bathsaturated by steady, regulated additions of aluminum chlorid, and thisproves to be a feature of distinct advantage and paramount im portance.I

My invention will be more readily understood by reference to theaccompanying drawings, in which:

Figure 1 is a more or less diagrammatic representation of the entiresystem of apparatus.

Fig. 2 is a sectional view, taken on a horizontal plane, of theelectrolyzing vat.

Figs. 3 and 4 are/other sectional views.

Referring first to" Fig. 1, it will be seen that the ChIOI'lIIlZ lIIQffurnace is shown at 9. The details of this furnace are unimportant inconnection with the present application and it suffices to say that acharge is, introduced into the chlorinizing furnfie. which is preferablyheated 'by electrical means. A pipe 30, which comesfrom a storage tank31. is led intothe chlorinizing furnace, as indicated in' the drawing,and

Patented Jan. 27, 1920.

aluminum therefrom and this carry out higher grades of'clay,

in this way the charge in the furnace is mediately effects thedisintegration of the kaolin, the

. the three gases which at a higher temperature formation of aluminumchlorid and silicon tetrachlorid, and, by the combination of the carbonandthe oxygen liberated' from the kaolin, the formation of carbonmonoxid.

The three gases thus formed naturally arise and pass out of thechlorinizing fur nace 9 and are conducted to a condenser 33. Thiscondenser is in the form of a double closed chamber providing thecompartment 34 and-the compartment 35, separated by a partition 36. Thecompartment 34 is provided with a system of. cooling pipes 37, 37, whichextend downwardly through and from the top tributed throughout theentire space of this particular compartment in order to get a completetemperature control. The pipes 37, 37 are joined at the upper end,outside of the chamber, by means of the header pipe 38, and circulationis secured in any desirable manner. In this particular condenser elementthe system of pipes is connected to a cold-v water supply and the resultis that as have been referred to enter and pass through the compartment34 the aluminum chlorid gas, which condenses than'the silicontetrachlorid gas, is condensed and deposits itself as a white powderupon the pipes Since the temperature which is produced by thecirculation of mere cold water in the cooling pipes 37, 37, is notsufiiciently low to condense silicon tetrachlorid, this gas, togetherwith the carbon monoxid, passes on to the next compartment 35 of thecondenser. Thus the first condenser element 34 is devoted to thecondensation of the aluminum 1 chlorid, and the white powder to which itis reduced is removed from the pipes upon which it is deposited by meansof the scrapers 39, 39. The powder is thus thrown down on to theconve'yer 42 and carried to a tank 45, the connection to which iscontrolled by a valve 46. It will be seen that this tank is connected bymeans of a pipe 47,

- with a compressed air tank 48, which is fed through the air compressor49. It is important, as before indicated, that the system be afclosedsystem and that various actions be carried on under pressure, and Ispeak of it particularly at this time because-of the fact that thealuminum chlorid to which I tetrachlorid gas of the chamber and whichare disv may be arranged to separate and the inclosure is effective incondensing and keeping condensed this volatile substance. 7

Leaving the aluminum chlorid, which has been deposited in the tank 45,for the prescut, I shall follow the-course of the silicon and the carbonmonoxid through the second element of the condenser. The condenserelement 35 is provided with a system of cooling pipes 50 like the pipes37, these pipes having the outside header 51 and being provided withscrapers 52, 52. Instead of being supplied with mere cold water,

however, the cooling pipes 50 are supplied with a freezing mixture oficewater and salt, and the temperature in the'condenser element 35 istherefore considerably lower than the temperature in the condenserelement 34. The lower temperature is sufiicient to condense the silicontetrachlorid, which comes down as a colorless liquid, except for anyimpurities which may-discolor. it. This liquid silicon tetrachloridpasses down the sloping bottom of the condenser element 35 and passesthrough the outlet 55, controlled by the valve 56, which leads to thetank 57. The tank 57 has an outlet pipe 57. r

The carbon monoxid passes out'of the con denser element 35 through apipe 59,- past a valve 60, into a closed gas pump 61, and'is pressuremay be kept upon the carbon monoXid which finds its way to this tank,and so that the carbon monoxid may be fed. by way of a pipe 66 to anynumber of burners 67, 68 and 69, which are used for heating purposes incertain other steps of the process which will hereinafter be referredto.

Where additional chlorids are formed in the chlorinizing furnace, whichcondense 'at other temperatures, as is the case when iron or titanium ispresent in clay, the condenser these from the aluminum and siliconchlorids and from each other if desired, by increasing the number ofelements maintained at different temperatures required to separatelydeposit the substances.

Returning now to the aluminum chlorid which has been deposited in theform of a powder in the tank 45 be noted that 1 have placed the burner67 under this tank, and I may mention here (this powder being whiteunless discolored by impurities) it will that I surround the tank with asuitable fire I can subject the tank to a high wall so that degree ofheat. With thevalve 46 closed, the material in the tank 45 can be placedunder high pressure from this pressure prevents the aluminum chlorid,melted by heat from the carbon monoxid burner, from vaporizing. Oncein-this c0ndition the aluminum chlorid is much more stable and much moreeasily handled, due to its physical condition, anddesirably so in viewof the steps which are to follow and which will presently be described.I desire to state, however, that it is entirely feasible to conduct thealuminum chlorid to the farther parts of the system in its dry,infusedstate, and I therefore do not wish to be limited to the inclusionof .this step of melting the aluminum chlorid.

A pipe leads from the tank 45 to avalve 71, which in turn is connectedwith a pipe 72 leading .into a furnace, preferably of the Rodenhauserthree-phase type. This furnace comprises a' a heavy outer housing whichis provided with a round bottom 74 mounted in a correspondingly shapedbase 75, the ideabeing that when the connecting pipes are temporarilydetached, the furnace can be tilted in order 'to ta off molten metal, aswill bepointed out a little later.

he lining ofthe furnace provides a cavity for the molten metal which isformed between and around tubular casing parts within which the magneticcircuit frame and the primary coils are'disnosed. The details of thisfurnace do not constitute part of my present invention, but I refer tothem because it is a type of furnace well adapted for use as part of mysystem. It will be seen that when the valve 71 is opened the liquidaluminum chlorid is conducted to the working chamber of the Rodenhauserfurnace. The reason for this step in the proc ess is as follows: Y

In the first condensation of the aluminum chlorid in the condenserelement 34, there are likely to be" impurities, iron, and it is theobject of process now under description to eliminate this iron and tosecure pure aluminum chlorid. Therefore, preliminaril Rodenhauserfurnace is charged with aluminum, and the molten bath, as illustrated,is formed when as before stated, the valve 71 is opened and the liquidaluminum chlorid is fed into this bath-of molten aluminum near thebottom thereof, the aluminum chlorid is immediately reconverted into agas due to the release of pressure and heat of bath, and passes upthrough the molten aluminum. Due to-the greater ailinity of the chlorinfor the aluminum than for the iron,'or other impurity for that matter,the chlorinreleases the iron and takes on the proper share of aluminum.

. The result is the tank 48, and.

84 is kept closed andthe principally the step'in the.

the

vet

that the refined aluminum chlorid will leave the bath of aluminum andwill pass out of the furnace throu h the pipe 81. It will 81 dividesinto the pipes 82 and 83, which are provided with valves 84 and 85,respectively. If the refined aluminum chlorid is to be further purified,the valve valve 85-is opened, so that the aluminum chlorid gas may passup the pipe 83 and be passed back into the condenser element 34 forcondensation purposes, and in its refined state it will be rechargedinto the Rodenha-user furnace, as has been described, and this processmay be repeated until the required degree of purity has been obtained.At this point the valve 85 is closed and the valve 84 is opened, so thatthe substantially pure aluminum chlorid may be passed into what'may betermed condenser #2, as indicated. This condenser is of the samestructure as the condenser element 34, and the condensed aluminumchlorid in the form of a white powder is brought down into the tank 86.

In this tank 86the aluminum chlorid mayv be put under pressure by way ofthe pipe 87 leading from the compressed-air tank 48, and may also besubjected to heat from a flame at the burner 69, preferably confinedwithin fire Walls. his again melts the aluminum chlorid, which may thenbe conducted to a storage tank 88 through a pipe 89 controlled by avalve 90, the pure aluminum chlorid being kept under the pressuretransmitted from the tank 86 and being heated by a carbonmonoxid flameat kept in a liquid This liquid condition is malntained by the heatwhich is developed by the electrolytic be noted that the pipe action.The electrolytic vat'is illustrated i indetail in Figs. 2, 3' and 4 andit will be seen that it comprises a graphite hearth 93' and firebricksurrounding walls 94, 94, with magnesite linings 95, 95, the entirebeing surounded by sustaining plates 96. Along opposite sides of the vatare access openings 97, 97*, which are normally sealed by means ofcovers 98, 98, and a tap hole 99 is provided for a purpose that will bereferred to presently, this tap hole be ing normally closed by meansofthe plug 100. A chlorin exit 101 ,is provided, and, as indicated inFig. 1, this exit is connected by means. of a pipe 102, in which thereis a valve 103, with .a chlorin compressor 104,

with a chlorin cooler 106, t ese two elements being merelydiagrammatically 30 eration, and, as

shown. The cooler 106 is connected by means of a pipe 107 with theliquidchlorin tank 31, which has already been referred to, and the connectingpipe 107 is provided with a valve 108.

Returning to the detailed showing of the electrolytic vat, it will beseen from Figs. 3 and 4 particularly, that the anodes are in the form ofgraphite blocks 109, to each of which three stems 110, 110, are secured,the

.stems being firmly lodged in a reinforced firebrick seal cover 111.'Each of the anodes is provided with a collar 112, which is engaged by aloose collar 113 which may be moved up and down by means of nuts 111'onbolt rods 115 extending upwardly from .a packing-box cover 116, whichsurrounds the electrode stem and packs it at 117. By this arrangementthe anode stems may be adjusted vertically so that the proper over-alladjustment may be secured within the vat. Copper bus bars 118, 118connect the tops of the electrode stems 110, and in this way the currentis conveyed to the bath, the graphite hearth acting as the oppositeelectrode. The center one of each set of three anode stems is drilledaxially,

as indicated at 110, and this bore is connected to distributingpassageways 120, 120 in the corresponding graphite block. Each of thesebores is connected by means of a pipe 121 with the supply pipe 92, whichhas been hereinbefore referred to, and a valve 122 is disposed in eachpipe 121 and is intermittently operated for feeding purposes by atraveler 123 which is mounted upon a rotating shaft 124. Thus, whenv thevarious rotating shafts 124. are put into opbefore stated, the valve '91is opened to permit the passage of the liquid aluminum chlorid, aconstant feed per unit of time is afforded down through the passageways119 and into the vat.

The liquid aluminum chlorid is kept at a high temperature, about 200degrees centigrade, and at about a pressure of two and a halfatmospheres. The heating of the storage tank is transmitted to hot-oilbaths in pipes 125 which surround the supply pipes 92, and thus it isinsured that the aluminum chlorid be fed into the vat at the propertemperature. The electrolyte is a bath of melted sodium chlorid at ahigh temperature which is primarily induced by external means, but whichis maintained by the application-of the current. Thealuminum chlorid isfed to the bath at such a rate as to keep the bath saturated. The

action which takes place in the electrolytic vat separates the aluminumfrom the chlorin and leaves the sodium chlorid. Due to the difference inspecific gravity between the pure aluminum which is thus obtained andthe melted sodium chlorid, it is a sim- 6b ple. matter to tap off themolten aluminum It will be seen that the process is uniquely continuous,and that the chlorin which is freed in the electrolytic vat may be usedover and over again in the chlorinizing furnace, while the carbonmonoxid which is formed by the oxygen liberated from the clay and thecoke which is introduced is used for burner purposes. 'It isimportantthat the system be a closed system, as described, to excludethe moisture and to protect the active chloride, particularly thealuminum chlorid. r i 1 An important feature in the matter of theoperation of my system is found in the feeding ofthe meltedaluminum'chlorid, or aluminum chlorid in powdered condition for thatmatter, to the electrolytic vat. It is of importance that theelectrolytic bath is fed with the aluminum chlorid in such a way as tokeep the bath saturated.

It will be apparent to those skilled in theart that variousmodifications might be made in this system without departing fromthespirit or scope thereof. For instance, one' might use a differentelectrolyte. In heating the pipes which maintain the aluminum chlorid inits melted conditionwhile being fed to the electrolytic bath, it mightbe better practice insome instances to use electric heating coils thanto use an'oil bath, and it might be well to heat the aluminum chloridcontainers in a manner other than by the carbon monoxid flame. With theclosed system which has been described, I have the particularadvantagethat there is no electrode consumption, and therefore when theelectrodes are adjusted they will remain adjusted, and economic serviceis secured.

Referring to the electrolytic vat, I may mention here that the hearth isthe cathode and the graphite blocks constitute the anode. The aluminumforms'globules varying in size from mere specks to considerably largerparticles, and they occur near the bottom and finally rest upon thebottom. The chlorin is liberated and streams away with great rapidity.The aluminum which is thus formed is heavier and settles tothe bottom,and the particles of aluminum as formed above the bottom frequently jointo form which, as described, is tapped out from the .vertical y intosaid chamber,

vat. It is'convenient to retain suflicient moltenaluminum in the vat tokeep the carbon cathode constantly covered.

It will appear that changes and modifications in the apparatus of myinvention will be possible Without departing from the spirit and scopeof my invention. I have already referred to the fact that the apparatusof my invention has much wider appllcation than for carrying out merelythe process which I have cited as an instance of use, and it is to beunderstood that I contemplate any use to which my apparatus may be put.I desire, therefore, that the metes' and bounds of my invention shall bedetermined by the appended claims, which I have drawn variously so as totions which, of their use,

I claim:

1. Apparatus for treating chlorid which of themselves, and regardlessare new.

comprises a closed chamber for containing an electrolyte having agraphite interior bottom as one electrode and a graphite block dependingfrom a sealed coveras the opposite electrode, and means for feedingmaterial into said electrolyte at a definite and controllable rateofspeed.

2. Apparatus for treating chlorid which comprises a closed chamber forcontainin an electrolyte, having a graphite interior bottom as oneelectrode anda graphite block depending from a sealed cover as theopposite electrode, and means for feeding material into said electrolytethrough abore insaid block at a definite and controllable rate of speed.

3. In combination, a chamber having a common electrode at the bottomthereof, a plurality of electrode mem-bers extending and a plurality ofhorizontal electrode members each common to a bers and connected theretoat the bottom thereof in horizontal position, being spaced properly awayfromsaid first-named electrode.

4. In combination, a chamber having a graphite bottomfor one electrodeand adapted to contain an electrolyte, a cover sealing said chamber, anelectrode passing through said cover, and means for adjusting thevertical position of said electrode, said elecbring out the combina-,

to be. treated to said chamber plurality of said first-named mem--members and connected thereto at the bot tom thereof in horizontalposition, being spaced properly away from said first-named electrode,said electrode members having passageways therethrough whereby saidchamber may be fed with material to be treated.

6. In combination, a chamber electrodeblock in the bottom thereof, aplurality; of, horizontal opposing electrode mem e-rs disposed in saidchamber, substantially parallel to said block, a plurality of verticalelectrodes extending upwardly from each ofsaid horizontal electrodes,one of each of said plurality of vertical electrodes having a passagewaytherethrough, each said passageway being supplemented by divergingbranches in the corresponding horizontal member.

7. Apparatus for treating chlorid which g ,comprises a closed chamberadapted to contain an electrolyte having a conducting interior bottom asone electrode and a c0nducting block depending from a sealed covermechanically feeding non-gaseous material into said electrolyte at adefinite and controllable rate of speed.

8. In combination,'a chamber adapted to contain an electrolyte,electrodes therein, and means for feeding non-gaseous material by aplurality of paths to distribute the feed uniformly throughout theelectrolyte.

9. In combination, a chamber adapted to contain an electrolyte,electrodes therein,

and means for feeding non-gaseous material to be treated to said chamberby a plurality of paths in substantially uniform relation to theelectrodes.

witness whereof, I my name this 2nd day of July, A. D. 1915.

VICTOR M. WEAVER.

having an as the opposite electrode, and means for hereunto subscribe

